JPH04202075A - Production of diamond coated hard material - Google Patents
Production of diamond coated hard materialInfo
- Publication number
- JPH04202075A JPH04202075A JP33422890A JP33422890A JPH04202075A JP H04202075 A JPH04202075 A JP H04202075A JP 33422890 A JP33422890 A JP 33422890A JP 33422890 A JP33422890 A JP 33422890A JP H04202075 A JPH04202075 A JP H04202075A
- Authority
- JP
- Japan
- Prior art keywords
- diamond
- acid
- sintered body
- coating layer
- alkali
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 43
- 239000010432 diamond Substances 0.000 title claims abstract description 43
- 239000000463 material Substances 0.000 title claims description 36
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- 239000011247 coating layer Substances 0.000 claims abstract description 24
- 239000002253 acid Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 17
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003513 alkali Substances 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 6
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 5
- 239000002585 base Substances 0.000 claims description 21
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 150000007513 acids Chemical class 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 4
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 2
- JUINSXZKUKVTMD-UHFFFAOYSA-N hydrogen azide Chemical compound N=[N+]=[N-] JUINSXZKUKVTMD-UHFFFAOYSA-N 0.000 claims 1
- 239000010410 layer Substances 0.000 abstract description 5
- 238000005268 plasma chemical vapour deposition Methods 0.000 abstract description 4
- 239000000853 adhesive Substances 0.000 abstract description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910021364 Al-Si alloy Inorganic materials 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000006061 abrasive grain Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、接着強度に優れたダイヤモンド被覆層を有す
るダイヤモンド被覆硬質材料の製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for manufacturing a diamond-coated hard material having a diamond coating layer with excellent adhesive strength.
超硬合金やセラミックス焼結体の基材表面に、ＰＶＤ法
やＯＶＤ法によりＴｉ、 Ｈｆ、 Ｚｒの炭化物、窒化
物又は炭窒化物、若しくはＡ１の酸化物等の硬質被覆層
を単層又は複層に形成した表面被覆硬質材料が、切削工
具や耐摩工具を始め、各種の機械用部品又は装飾品とし
て広く利用されている。A hard coating layer such as a carbide, nitride or carbonitride of Ti, Hf, or Zr, or an oxide of A1 is applied to the surface of a base material of a cemented carbide or a ceramic sintered body by a PVD method or an OVD method. Surface-coated hard materials formed in layers are widely used as cutting tools, wear-resistant tools, various mechanical parts, or decorative items.
最近では、これら表面被覆硬質材料の被覆層として、硬
度が極めて高く、化学的に安定であり、高い熱伝導率や
音波伝播速度を始めとする数多くの優れた特性を供えた
ダイヤモンドが注目され、多くの分野で実用化されてい
る。例えば、ダイヤモンド被覆したスローアウェイチッ
プ、ドリル、マイクロドリル、エンドミル等のダイヤモ
ンド被覆切削工具は、Ａ１やＣｕ又はこれらの合金等を
高速で切削でき、被削材の仕上げ面が極めて良好である
。又、耐摩工具のひとつであるダイヤモンド被覆したボ
ンディングツールにより、半導体装置のワイヤボンディ
ングが高い寸法精度で長時間実施出来るようになってい
る。Recently, diamond has attracted attention as a coating layer for these surface-coated hard materials, as it has many excellent properties such as extremely high hardness, chemical stability, high thermal conductivity, and sound propagation speed. It has been put into practical use in many fields. For example, diamond-coated cutting tools such as diamond-coated indexable tips, drills, micro drills, and end mills can cut A1, Cu, or their alloys at high speed, and the finished surface of the workpiece is extremely good. Furthermore, diamond-coated bonding tools, which are one type of wear-resistant tool, have enabled wire bonding of semiconductor devices to be carried out for long periods of time with high dimensional accuracy.
これらダイヤモンド被覆硬質材料のダイヤモンド被覆層
を形成する方法としては、マイクロ波プラズマＯＶＤ法
、ＲＦプラズマＣｖＤ法、ＥＡ−ＯＶＤ法、誘磁場マイ
クロ波プラズマＣｖＤ法、ＲＦ熱ブラズ？ＯＶＤ法、Ｄ
ＣプラズマＣｖＤ法、ＤｏブラスマジェットＯＶＤ法、
熱フィラメントＯＶＤ法、燃焼法など数多くの方法が知
られている。又、ＰｖＤ法によればダイヤモンド状カー
ボンを主に形成することが出来る。Methods for forming the diamond coating layer of these diamond-coated hard materials include microwave plasma OVD, RF plasma CvD, EA-OVD, induced magnetic field microwave plasma CvD, and RF thermal plasma CVD. OVD method, D
C plasma CvD method, Do plasma jet OVD method,
Many methods are known, such as the hot filament OVD method and the combustion method. Further, according to the PvD method, diamond-like carbon can be mainly formed.
ところが、ダイヤモンド被覆硬質材料の多くは基材とダ
イヤモンド被覆層の密着弾度が不足しているため、層剥
離により寿命に至る場合が多い。However, in most diamond-coated hard materials, the adhesion elasticity between the base material and the diamond coating layer is insufficient, and thus the life of the diamond-coated hard material is often reached by delamination.
この原因として、次の３つが考えられる：■ダイヤモン
ドと基材の熱膨張係数が大きく異なるため、ダイヤモン
ド被覆層中に残留応力が発生している。There are three possible causes for this: ■ Residual stress is generated in the diamond coating layer because the thermal expansion coefficients of the diamond and the base material are significantly different.
■炭素の拡散が容易なＦｅやＣｏ等の金属元素を含む超
硬合金が基材である場合、これら金属元素上に密着強度
を低下させるグラファイトが優先的に生成する。(2) When the base material is a cemented carbide containing metal elements such as Fe and Co through which carbon can easily diffuse, graphite, which reduces adhesion strength, is preferentially formed on these metal elements.
■ダイヤモンドが極めて安定なため、基材との接合が密
着強度の低い分子間引力による。■Because diamond is extremely stable, bonding with the base material is based on intermolecular attraction with low adhesion strength.
これに対して、ダイヤモンド被覆層の密着強度を改善向
上させるため、以下のような試みが従来から行われてい
る：
前記■の原因に対しては、特開昭６１−２９１４９３号
公報に記載の如く、ダイヤモンドと近似する熱膨・張係
数を持つ窒化ケイ素（ｓ、ｔ Ｎ ）又は炭化ケイ素（
Ｓ、ｔａ）を主成分とする焼結体を基材として用いる方
法。In order to improve and improve the adhesion strength of the diamond coating layer, the following attempts have been made in the past: For the cause of the above (■), the method described in Japanese Patent Application Laid-Open No. 61-291493 has been made. Silicon nitride (s, t N ) or silicon carbide (
A method using a sintered body containing S, ta) as a base material.
前記■の原因に対しては、特開平］、 −２０１４７５
号公報に記載の如く、超硬合金表面を酸溶液でエツチン
グしてＦｅやＣｏ等の金属元素を除去する方法。Regarding the cause of the above-mentioned ■, Japanese Patent Application Laid-open No. 2014-201475
As described in the above publication, a method of etching the cemented carbide surface with an acid solution to remove metal elements such as Fe and Co.
前記■の原因に対しては、特開昭６１−１２４５７３号
公報に記載の如く、ダイヤモンド砥粒又は砥石により基
材表面に傷つけ処理を行って０．２〜１０μｍ程度の凹
凸を付け、ダイヤモンドの核発生密度を向上させる方法
。As for the cause of the above (1), as described in JP-A No. 61-124573, the surface of the base material is scratched with diamond abrasive grains or a grindstone to create irregularities of about 0.2 to 10 μm, and the diamond How to improve nucleation density.
しかし、上記したいずれの方法によっても、切削工具や
耐摩工具として充分な密着強度を備えたダイヤモンド被
覆硬質材料を得ることが困難であった。However, by any of the above-mentioned methods, it has been difficult to obtain a diamond-coated hard material with sufficient adhesion strength as a cutting tool or a wear-resistant tool.
本発明はかかる従来の事情に鑑み、熱膨張係数がダイヤ
モンドに近いＳｉ Ｎ を主成分とする焼結体を基材と
し、その表面に密着強度に優れたダイヤモンド被覆層を
形成することを目的とする。In view of such conventional circumstances, the present invention aims to form a diamond coating layer with excellent adhesion strength on the surface of a sintered body mainly composed of SiN, which has a coefficient of thermal expansion close to that of diamond. do.
上記目的を達成するため、本発明にあっては、窒化ケイ
素を主成分とする焼結体からなる基材の表面にダイヤモ
ンド又はダイヤモンド状カーボンの被覆層を形成するダ
イヤモンド被覆硬質材料の製造方法において、前記基材
の表面を５重量％以上のフッ酸又はフッ硝酸の水溶液、
１０重量％以上の前記酸以外の酸又はアルカリの水溶液
、若しくは溶融水酸化ナトリウムに浸漬若しくは接触さ
せた後、該表面に前記被覆層を形成するこ左を特徴とす
る。In order to achieve the above object, the present invention provides a method for manufacturing a diamond-coated hard material in which a coating layer of diamond or diamond-like carbon is formed on the surface of a base material made of a sintered body mainly composed of silicon nitride. , the surface of the base material is coated with an aqueous solution of 5% by weight or more of hydrofluoric acid or hydrofluoronitric acid,
The coating layer is formed on the surface after being immersed in or brought into contact with an aqueous solution of an acid or alkali other than the above acid or molten sodium hydroxide in an amount of 10% by weight or more.
従来から、Ｓｉ Ｎ を主成分とする焼結体（ＳｉＮ
基焼結体）は、一般に酸やアルカリによってエツチング
されないことが特徴とされていた。Conventionally, sintered bodies mainly composed of SiN (SiN
The base sintered body) was generally characterized by not being etched by acids or alkalis.
然るに本発明者等の研究によれば、Ｓｉ Ｎ 粉末の焼
結性を改善するためにＡＩ Ｏ、Ｙ Ｏ、ＭｇＯ，Ａ７
Ｎ、 ＳｉＯ等の焼結助剤を添加して焼結したＳｉ Ｍ
基焼結体は、強酸や強アルカリによって僅かながら腐食
され、表面に微小な凹凸が形成されることが判った。こ
れは、表面の粒界及び粒界近傍のガラス質が優先的に腐
食され、ＳｉＨの柱状結晶が残るためと考えられる。し
かも、この腐食は表面の一定深さに止まり深い亀裂や溝
状になることがないので、ＳｉＮ 基焼結体が腐食によ
って基材としての強度を低下させることはなかった。However, according to the research of the present inventors, in order to improve the sinterability of Si N powder, AI O, Y O, MgO, A7
SiM sintered with addition of sintering aids such as N and SiO
It was found that the base sintered body was slightly corroded by strong acids and strong alkalis, and minute irregularities were formed on the surface. This is thought to be because the grain boundaries on the surface and the vitreous material near the grain boundaries are preferentially corroded, leaving columnar SiH crystals. Furthermore, since this corrosion was limited to a certain depth on the surface and did not form deep cracks or grooves, the strength of the SiN-based sintered body as a base material did not decrease due to corrosion.
Ｓｉ Ｎ 基焼結体の表面を上記の如く腐食する為に
は、酸の水溶液としては５重量％以上のフツ酸又はフッ
硝酸の水溶液、あるいはフン酸又はフッ硝酸以外の酸、
例えば塩酸、硫酸、硝酸、リン酸等の１０重量％以上の
水溶液を用いる。又、例えば水酸化カリウム、水酸化ナ
トリウム、炭酸ナトリウム等のアルカリの水溶液の場合
も１０重量％以上の水溶液を用いる。これら酸又はアル
カリの水溶液が上記濃度未満の場合には、Ｓｉ Ｎ
基焼結体を長期間浸漬しても表面状態が変化しない。In order to corrode the surface of the SiN-based sintered body as described above, the aqueous acid solution should be an aqueous solution of 5% by weight or more of hydrofluoric acid or fluoronitric acid, or an acid other than hydrofluoric acid or fluoronitric acid.
For example, an aqueous solution of 10% by weight or more of hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, etc. is used. Also, in the case of an aqueous alkali solution such as potassium hydroxide, sodium hydroxide, sodium carbonate, etc., an aqueous solution of 10% by weight or more is used. When the aqueous solution of these acids or alkalis is less than the above concentration, SiN
The surface condition does not change even if the base sintered body is immersed for a long period of time.
特に、溶融水酸化す） ＩＪウムにＳｉ Ｎ 基焼結
体を接触させると、ＳｉＮ も一部腐食されて表面粗
さＲが１０μｍ又はそれ以上となるので、ダイａｘ
ヤモンド被覆層の密着強度向上に大きく、寄与すること
が判った。In particular, when a SiN-based sintered body is brought into contact with molten hydroxide (IJ), some of the SiN is also corroded and the surface roughness R becomes 10 μm or more, which improves the adhesion strength of the diamond coating layer. It was found that it significantly contributed to
又、上記焼結体を、酸の水溶液と、アルカリの水溶液又
は溶融水酸化す） ＩＪウムとに順番に浸漬又は接触さ
せれば、更に良好な被覆層の密着強度が得られることが
判った。これは、酸により優先的に腐食されるものと、
アルカリにより優先的に腐食されるものとがあるためと
考えられる。Furthermore, it has been found that even better adhesion strength of the coating layer can be obtained by immersing or contacting the above sintered body in an acid aqueous solution, an alkali aqueous solution, or molten IJum in order. . These are those that are preferentially corroded by acids, and those that are preferentially corroded by acids.
This is thought to be because some materials are preferentially corroded by alkali.
上記の如く本発明方法により表面を腐食した５１Ｎ４基
焼結体を基材とすれば、表面に５１３Ｎ、の柱状晶が存
在し且つ微細な凹凸が形成されているので、基材へのダ
イヤモンド被覆層の密着強度が従来に比べて飛躍的に向
上する。しかも、上記腐食によりガラス質が除かれ表面
でのＳｉ Ｎ の面積率が増加するので、基材表面の
熱膨張係数が一層ダイヤモンドに近付くことになり、熱
残留応力の発生が小さくなるから、この点からもダイヤ
モンド被覆層の密着強度が向上する。As described above, if a 51N4-based sintered body whose surface has been corroded by the method of the present invention is used as a base material, there are columnar crystals of 513N on the surface and fine irregularities are formed, so it is difficult to coat the base material with diamond. The adhesion strength of the layers is dramatically improved compared to conventional methods. Furthermore, as the glassy substance is removed by the above corrosion and the area ratio of SiN on the surface increases, the coefficient of thermal expansion of the base material surface becomes closer to that of diamond, and the generation of thermal residual stress becomes smaller. This also improves the adhesion strength of the diamond coating layer.
尚、ダイヤモンド被覆層に関しては、層厚が０．１μｍ
未満では被覆層による耐摩耗性などの諸性質の向上が認
められず、又層厚２００μｍを超える被覆層を形成して
も大きな性能の向上がもはや認められないので、０．１
〜２００μｍの層厚が好ましい。As for the diamond coating layer, the layer thickness is 0.1 μm.
If the thickness is less than 0.1, no improvement in various properties such as abrasion resistance due to the coating layer will be observed, and even if a coating layer with a thickness exceeding 200 μm is formed, no significant improvement in performance will be observed.
Layer thicknesses of ˜200 μm are preferred.
組成がＳｉ Ｎ −４ｗｔ％ＡＩ Ｏ−４ｗｔ％ＺｒＯ
−３ｗｔ％Ｙ ＯのＳｉ Ｎ 基焼結体を１．Ｔ工Ｓ
で定められた５ＰＧＮ １２０３０８の形状で、刃先処
理として一般に行われているネガランド（以下Ｎ、Ｌと
呼ぶ）を施したスローアウェイチップに加工した。尚、
刃先処理の処理角度は２５°、処理量はＱ、ｌａｗとし
た。Composition is SiN-4wt%AIO-4wt%ZrO
A Si N -based sintered body containing -3 wt% YO was prepared in 1. T-engine S
The indexable tip was processed into an indexable tip having the shape of 5PGN 120308 defined by the following, and subjected to a negative land (hereinafter referred to as N and L), which is generally performed as a cutting edge treatment. still,
The processing angle of the blade edge processing was 25°, and the processing amount was Q, law.
得られた複数のチップを、下表に示す前処理液に浸漬又
は接触させた。前処理条件は、酸又はアルカリの水溶液
には５０Ｃで１０分間浸漬し、溶融ＮａＯＨの場合は固
体ＮａＯＨを６００Ｃで加熱溶融したものに２分間接触
させた。前処理後、被覆層形成初期におけるダイヤモン
ド核の発生密度を向上させるため、３μｍ以下のダイヤ
モンドペーストでチップ全面を１０分間傷付は処理した
。A plurality of the obtained chips were immersed in or brought into contact with the pretreatment liquid shown in the table below. The pretreatment conditions were immersion in an acid or alkali aqueous solution at 50C for 10 minutes, and in the case of molten NaOH, contact with solid NaOH heated and melted at 600C for 2 minutes. After the pretreatment, the entire surface of the chip was scratched for 10 minutes with a diamond paste of 3 μm or less in order to improve the density of diamond nuclei generated at the initial stage of coating layer formation.
次に、各チップを２．４５ＧＨｚのμ被プラズマＣＶＤ
装置にセットし、１０００ Ｃ＆、；加熱し、全圧１０
０ｔｏｒｒとしたＨ−１，５％ＯＨの混合プラズマ中に
４〜１００時間保持して、チップの上面全体、逃げ面の
切れ刃近傍及びＮＬ面にダイヤモンド被覆層を形成する
ことにより、本発明チップの試料１〜１２を作製した。Next, each chip was subjected to 2.45 GHz μ plasma CVD.
Set it in the device, heat it to 1000C, and bring the total pressure to 10
The chip of the present invention is maintained in a mixed plasma of H-1,5% OH at 0 torr for 4 to 100 hours to form a diamond coating layer on the entire upper surface of the chip, near the cutting edge of the flank face, and on the NL surface. Samples 1 to 12 were prepared.
比較のため、上記と同一組成のＳｉ Ｎ 基焼結体から
なる同一形状のスローアウェイチップで、上下面及び逃
げ面ともに研削した比較チップの試料１、並びにこれに
更にダイヤモンドペーストでチップ全面を３０分間傷付
は処理した後、上記と同様にダイヤモンド被覆層を形成
した比較チップの試料２を準備した。For comparison, sample 1 is an indexable tip of the same shape made of a Si N -based sintered body with the same composition as above, which is a comparison tip whose top and bottom surfaces and flank surfaces are both ground. After treating the scratches for a minute, a comparative chip sample 2 was prepared with a diamond coating layer formed thereon in the same manner as above.
尚、形成したダイヤモンド被覆層については、ラマン分
光分析法によってダイヤモンドの特徴である１３３３ｃ
ｍ のピークを確認した。The formed diamond coating layer was found to be 1333c, which is a characteristic of diamond, by Raman spectroscopy.
A peak of m was confirmed.
得られた各チップについて、
被削材 ： Ａｌ−１４ｗｔ％Ｓ１合金の溝入り材切削
速度： ５００ｍ／ｍｉｎ
送 リ ＝ ０．２ ｒｎｒＶ′ｒｅ
ｖ切り込み：１．Ｑｍｍ
切削時間：３０分
の条件での乾式断続切削試験と、並びに被削材 ： Ａ
１．−１７ｗｔ％８１合金の丸棒材切削速度： ２００
ｍ／ｍｉｎ
送 リ ：０．４ｍ与／ｒｅＶ切り込み
＝１．０問
切削時間＝５分
の条件での乾式連続切削試験を行い、切れ刃１０個の平
均逃げ面摩耗量、及びダイヤモンド被ＭＮの剥離発生切
れ刃数を測定した。For each chip obtained, Work material: Grooved material of Al-14wt%S1 alloy Cutting speed: 500 m/min Feed rate = 0.2 rnrV're
v cut: 1. Qmm Cutting time: Dry interrupted cutting test under conditions of 30 minutes, and work material: A
1. -17wt%81 alloy round bar cutting speed: 200
A dry continuous cutting test was conducted under the conditions of m/min feed rate: 0.4 m given/reV depth of cut = 1.0 questions, cutting time = 5 minutes, and the average flank wear amount of 10 cutting edges and the diamond-covered MN The number of cutting edges at which peeling occurred was measured.
結果を下表に併せて示した。The results are also shown in the table below.
上記の結果から、本発明チップはいずれも従来例である
比較チップより優れた耐摩耗性と耐剥離性を備えること
、特にフッ酸やフツ硝酸並びに溶融ＮａＯＨで処理した
本発明チップは他よりも優れていることが判る。From the above results, it can be seen that all of the chips of the present invention have better wear resistance and peeling resistance than the comparative chips, which are conventional examples.In particular, the chips of the present invention treated with hydrofluoric acid, hydrofluoric nitric acid, and molten NaOH are better than other chips. It turns out to be excellent.
本発明によれば、熱膨張係数がダイヤモンドに近いＳｉ
Ｎ 基焼結体を基材とし、簡単な前処理によって基材
表面に密着強度に優れたダイヤモンド被覆層を形成する
ことが出来る。According to the present invention, Si has a coefficient of thermal expansion close to that of diamond.
Using an N-based sintered body as a base material, a diamond coating layer with excellent adhesion strength can be formed on the surface of the base material through simple pretreatment.
従って、本発明によるダイヤモンド被覆硬質材料は、切
削工具としてＡｌ−Ｓｉ系合金の重切削においても良好
な耐摩耗性を示しミ長期間の使用が可能となるほか、耐
摩工具としてもダイヤモンド被覆層が剥離しにくく長期
間安定して使用出来る。Therefore, the diamond-coated hard material according to the present invention exhibits good wear resistance even in heavy cutting of Al-Si alloys as a cutting tool, and can be used for a long period of time. It does not easily peel off and can be used stably for a long period of time.
Claims (2)
表面にダイヤモンド又はダイヤモンド状カーボンの被覆
層を形成するダイヤモンド被覆硬質材料の製造方法にお
いて、前記基材の表面を５重量％以上のフツ酸又はフツ
硝酸の水溶液、１０重量％以上の前記酸以外の酸又はア
ルカリの水溶液、若しくは溶融水酸化ナトリウムに浸漬
若しくは接触させた後、該表面に前記被覆層を形成する
ことを特徴とする前記ダイヤモンド被覆硬質材料の製造
方法。(1) In a method for producing a diamond-coated hard material, in which a diamond or diamond-like carbon coating layer is formed on the surface of a base material made of a sintered body mainly composed of silicon nitride, the surface of the base material is 5% by weight or more. The coating layer is formed on the surface after immersion in or contact with an aqueous solution of hydrofluoric acid or hydronitric acid, an aqueous solution of an acid or alkali other than the above acid of 10% by weight or more, or molten sodium hydroxide. A method for producing the diamond-coated hard material.
、アルカリの水溶液又は溶融水酸化ナトリウムとに、順
番に浸漬又は接触させることを特徴とする、請求項（１
）記載のダイヤモンド被覆硬質材料の製造方法。(2) Claim (1) characterized in that the surface of the base material is immersed or brought into contact with an aqueous solution of any of the acids and an aqueous alkali solution or molten sodium hydroxide in order.
) The method for manufacturing the diamond-coated hard material described in .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33422890A JPH04202075A (en) | 1990-11-30 | 1990-11-30 | Production of diamond coated hard material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33422890A JPH04202075A (en) | 1990-11-30 | 1990-11-30 | Production of diamond coated hard material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04202075A true JPH04202075A (en) | 1992-07-22 |
Family
ID=18274983
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP33422890A Pending JPH04202075A (en) | 1990-11-30 | 1990-11-30 | Production of diamond coated hard material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04202075A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2686599A1 (en) * | 1992-01-28 | 1993-07-30 | Ngk Spark Plug Co | PROCESS FOR PRODUCING A SILICON NITRIDE ARTICLE COATED WITH A DIAMOND FILM OR SIMILAR MATERIAL |
| EP0700033A3 (en) * | 1994-08-26 | 1996-05-22 | Aiwa Co | Side-mounted thin film magnetic head and method of fabrication thereof |
| EP1138656A1 (en) | 2000-03-31 | 2001-10-04 | Ngk Spark Plug Co., Ltd. | Silicon nitride member, method for manufacturing the same, and cutting tool |
-
1990
- 1990-11-30 JP JP33422890A patent/JPH04202075A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2686599A1 (en) * | 1992-01-28 | 1993-07-30 | Ngk Spark Plug Co | PROCESS FOR PRODUCING A SILICON NITRIDE ARTICLE COATED WITH A DIAMOND FILM OR SIMILAR MATERIAL |
| EP0700033A3 (en) * | 1994-08-26 | 1996-05-22 | Aiwa Co | Side-mounted thin film magnetic head and method of fabrication thereof |
| US5777824A (en) * | 1994-08-26 | 1998-07-07 | Aiwa Research And Development, Inc. | Side-disposed thin film magnetic head and method of fabrication thereof |
| EP1138656A1 (en) | 2000-03-31 | 2001-10-04 | Ngk Spark Plug Co., Ltd. | Silicon nitride member, method for manufacturing the same, and cutting tool |
| US6863963B2 (en) | 2000-03-31 | 2005-03-08 | Ngk Spark Plug Co., Ltd. | Silicon nitride member, method for manufacturing the same, and cutting tool |
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